反应详情

Charge a 50 mL round bottom flask equipped with: a magnetic stirrer, temperature controlled heating mantle, N2 atmosphere, condenser, with 7-chloro-3-iodo-imidazo[1,2-a]pyridine (1.0 g, 3.6 mmol), 4-(hydroxymethyl)phenyl boronic acid (570 mg, 3.75 mmol), 2 M K2CO3 (7 mL), dimethoxy ethane DME (25 mL). Deoxygenate with a nitrogen purge and add Pd(TPP)4 (200 mg, 0.17 mmol 5 mol %) and heat the reaction to 65° C. for 48 hours. Cool the reaction and siphon off the lower aqueous phase (5 mL). Evaporate the reaction under vacuum at 42° C. to remove DME. Take up the residue in CH2Cl2 and wash with water (15 mL). Concentrate the CH2Cl2 and chromatograph giving an oil that solidified on standing to an ivory solid 670 mg (72%) MS (ES), m/z 259.1 (M+1).

1. additionCharge a 50 mL round bottom flask
2. customequipped with: a magnetic stirrer
3. customDeoxygenate with a nitrogen
4. custompurge
5. temperatureheat
6. customthe reaction to 65° C. for 48 hours
7. temperatureCool
8. customEvaporate
9. customthe reaction under vacuum at 42° C.
10. customto remove DME
11. washwash with water (15 mL)
12. concentrationConcentrate the CH2Cl2 and chromatograph
13. customgiving an oil that